di-tert-butyl alpha,alpha,alpha',alpha'-tetramethyl-(p-phenylenedimethylene) diperoxide synthesis

Yield:-

Reaction Conditions:

with sulfuric acid;sodium perchlorate at 25 - 45; for 0.5 h;

Steps:

1.1; 1.2; 1.3; 1.4; 1.5; 1.6; 1.7

Step 1. According to the ratio of addition, meta+para-2-propenyl alcohol:Tert-butyl hydroperoxide = 1 mol: 2.3 mol, the raw material 70% t-butyl hydroperoxide was metered into the condensation reaction vessel, stirred well, the temperature was maintained at 25 ° C; Step 2, under sufficient agitation,The raw material meta+para-2-propiophenol is metered into the condensation reactor and stirred well; the temperature is maintained at 25 ° C; Step 3, according to the weight ratio, meta+para-2-propenyl alcohol: 70% sulfuric acid:Sodium perchlorate = 100:1:0.5, adding a metered solid sodium perchlorate to the condensation reactor,Stir well, add a metered 70% sulfuric acid solution, stir well; keep the temperature at 30 ° C; Step 4, according to the weight ratio, meta+para-2-propenyl alcohol: 7 accelerator=100:30,The metered 7 accelerator is gradually added to the condensation reactor.At the same time, gradually increase the reaction temperature 35 ° C → 40 ° C → 45 ° C → 50 ° C → 55 ° C, after the 7 accelerator is gradually added, the reaction temperature is maintained at 45 ° C; Step 5, keep stirring thoroughly, keep the reaction temperature at 45 ° C, and keep under normal pressure conditions.The reaction is continued for 30 minutes, and the condensation reaction can be completed; Step 6. After the reaction is completed, according to the weight ratio, meta+para-2-propenyl alcohol:30% NaOH = 100:5, add metered pure water, reduce the temperature to 40 ° C,Add a metered 30% NaOH,Performing alkali washing and water washing; discharging the reaction wastewater into the wastewater collecting tank; Step 7. The meta-position + para-di-(tert-butylperoxyisopropyl) after washing the alkali with waterThe benzene product was transferred to a desiccator, dried by bubbling dry N2, and kept at a drying temperature of 50 ° C.Under normal pressure conditions, a qualified meta+di-di-(tert-butylperoxyisopropyl)benzene product is finally obtained.

References:

CN108929257,2018,A Location in patent:Paragraph 0014; 0016-0024